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High-temperature resistant modified silicon-containing cyanate ester resin as well as preparation method and application thereof

a technology of modified silicon and cyanate ester, which is applied in the field of polymer materials, can solve the problems of poor tensile strength and toughness, poor interfacial properties, and low heat resistance of general epoxy resin systems, and achieve the effect of heat resistance enhancement and resin heat resistan

Active Publication Date: 2018-09-06
SUZHOU TAIHU ELECTRIC ADVANCED MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The present invention provides a high-temperature resistant modified silicon-containing cyanate ester resin that can meet the resin viscosity requirement for pultrusion molding and enhance toughness and heat resistance of the resins. This is achieved by using a new-generation cyanate ester resin with low price and high heat resistance, and by improving flexibility and glass transition temperature of the resin through the use of epoxy-containing silsesquioxane. A high-temperature resistant resin composition with excellent heat resistance and good cost advantages can be prepared. The resin composition has low viscosity and good properties, which meets the requirements for pultrusion molding without needing an additional diluent.

Problems solved by technology

At present, common resins belong to an epoxy resin system, while a general epoxy resin system has a defect of low heat resistance.
Although partial resins have good heat resistance, the glass-transition temperature Tg of a cured matter is generally not higher than 180° C., interfacial properties are poor, and tensile strength and toughness are poor.
Although high heat resistance may be obtained by modifying the general epoxy resin, the general epoxy resin is difficult to be applicable to large-scale production due to limited raw materials and a complicated manufacturing process.
Although the cyanate ester resin has extremely high heat resistance, toughness of the cyanate ester resin is insufficient due to a limitation of the own structure, and the cyanate ester resin is difficult to be directly applied to a pultrusion process.
In a traditional modification method, an additional toughening agent or resin is adopted for compounding, but such a method may bring influences that the glass-transition temperature is decreased and partial mechanical properties and electrical properties are reduced.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

embodiment 1

[0032]steps: (a) adding 400 g of n-butyl alcohol and 20 g of tetramethylammonium hydroxide aqueous solution (with a mass fraction of 10%) into 1000 mL of three-mouth flask with a thermometer and a condensing tube, stirring and mixing uniformly, dropping 20 g of hydroxyl-terminated polydimethylsiloxane and a mixed solution of 120 g of γ-(2,3-epoxypropoxy) propyl trimethoxysilane and 80 g of ethanol into the above solution, controlling a dropping speed to complete dropping within 3 h, controlling a reaction temperature to 10° C., performing hydrolytic polycondensation for 6 h, and distilling off residual solvent and small molecules in the system by a rotary evaporator after the reaction is ended, thereby obtaining transparent viscous liquid capable of flowing at a room temperature for later use, i.e., the epoxy-containing silsesquioxane (G-POSS);

[0033](b) pouring 30 g of the viscous liquid (G-POSS) and 270 g of bisphenol A cyanate ester resin into 500 mL of three-mouth flask and stirr...

embodiment 2

[0036]steps: (a) adding 400 g of n-butyl alcohol and 20 g of tetramethylammonium hydroxide aqueous solution (with a mass fraction of 10%) into 1000 mL of three-mouth flask with a thermometer and a condensing tube, stirring and mixing uniformly, dropping 20 g of hydroxyl-terminated polydimethylsiloxane and a mixed solution of 120 g of γ-(2,3-epoxypropoxy) propyl trimethoxysilane and 80 g of ethanol into the above solution, controlling a dropping speed to complete dropping within 3 h, controlling a reaction temperature to 10° C., performing hydrolytic polycondensation for 6 h, and distilling off residual solvent and small molecules in the system by a rotary evaporator after the reaction is ended, thereby obtaining transparent viscous liquid capable of flowing at a room temperature for later use, i.e., a final product of epoxy-containing silsesquioxane (G-POSS);

[0037](b) pouring 30 g of the viscous liquid (G-POSS) and 270 g of bisphenol F cyanate ester resin into 500 mL of three-mouth ...

embodiment 3

[0040]steps: (a) adding 400 g of n-butyl alcohol and 16 g of tetramethylammonium hydroxide aqueous solution (with a mass fraction of 10%) into 1000 mL of three-mouth flask with a thermometer and a condensing tube, stirring and mixing uniformly, dropping 26 g of hydroxyl-terminated polydimethylsiloxane and a mixed solution of 127 g of γ-(2,3-epoxypropoxy) propyl trimethoxysilane and 90 g of ethanol into the above solution, controlling a dropping speed to complete dropping within 3.5 h, controlling a reaction temperature to 10° C., performing hydrolytic polycondensation for 5 h, and distilling off residual solvent and small molecules in the system by a rotary evaporator after the reaction is ended, thereby obtaining transparent viscous liquid capable of flowing at a room temperature for later use, i.e., a final product of epoxy-containing silsesquioxane (G-POSS);

[0041](b) pouring 30 g of the viscous liquid (G-POSS) and 270 g of bisphenol F cyanate ester resin into 500 mL of three-mout...

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Abstract

The present invention relates to a high-temperature resistant modified silicon-containing cyanate ester resin as well as a preparation method and an application thereof. The preparation method comprises the following steps: adding a mixed solution of hydroxyl silicone oil, a silane coupling agent and an organic solvent into a mixed solution of a tetramethylammonium hydroxide aqueous solution and a polar solvent, performing hydrolytic polycondensation at a temperature of 5-40° C. for 4-8 h, and performing distillation to obtain an epoxy-containing silsesquioxane; performing pre-polymerization on the epoxy-containing silsesquioxane and a cyanate ester resin at a temperature of 50-100° C. for 1-8 h to obtain a modified cyanate ester resin; and uniformly mixing the modified cyanate ester resin and a modified anhydride, thereby obtaining the high-temperature resistant modified silicon-containing cyanate ester resin.

Description

CROSS-REFERENCE TO RELATED APPLICATIONS[0001]This application is a continuation of International Patent Application No. PCT / CN2016 / 096229 with a filing date of Aug. 22, 2016, designating the United States, now pending, and further claims priority to Chinese Patent Application No. 201510746188.9 with a filing date of Nov. 6, 2015. The content of the aforementioned applications, including any intervening amendments thereto, are incorporated herein by reference.TECHNICAL FIELD[0002]The present invention belongs to the technical field of polymer materials, and particularly relates to a high-temperature resistant modified silicon-containing cyanate ester resin as well as a preparation method and an application thereof.BACKGROUND OF THE PRESENT INVENTION[0003]A uniform solidified core layer formed by compounding carbon fibers and resins is arranged inside a carbon fiber compound core conductor, while the material has extremely high requirements for a curing speed, glass-transition tempera...

Claims

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Application Information

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IPC IPC(8): C08G73/06C08G77/452C08G81/02C08G59/32
CPCC08G73/0644C08G77/452C08G81/025C08G59/3281C08K3/04C08G77/14C08L83/06C08G73/065C08G81/024
Inventor WU, BINZHANG, CHUNQIGU, JIANFENGJING, FENGXIQIU, FENGXIA, ZHIFENGMA, JUNFENG
Owner SUZHOU TAIHU ELECTRIC ADVANCED MATERIAL CO LTD
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